Synthesis of Co3O4 nanoparticles via the CTAB-assisted method

Cobalt oxide (Co₃O₄) nanoparticles were successfully synthesized by the cetyltrimethylammonium bromide (CTAB)-assisted method at normal pressure for the first time. The structure and morphology of the as-prepared Co₃O₄ nanoparticles were characterized by powder X-ray diffracton (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and N₂-sorption analysis. XRD studies indicated that the as-prepared product was well-crystallized cubic phase of Co₃O₄ with a cell constant of α = 8.0722 Å. The EM images showed that the obtained Co₃O₄ sample consisted of dispersive quasi-spherical particles with the size ranged from 15 to 25 nm.     

Synthesis and characterization of Co3O4 hollow spheres

Co₃O₄ hollow spheres were hydrothermally prepared at 130 °C for 16 h in the presence of Poly-vinylpyrrolidone (PVP). The as-prepared products were characterized by powder X-ray diffraction (XRD), field-emission scanning electron microscope (FE-SEM), transmission electron microscopy (TEM), infrared spectrum (IR), X-ray photoelectron spectrum (XPS), and optical absorption spectrum. PVP surfactant plays important roles in the formation of Co₃O₄ hollow spheres. These Co₃O₄ hollow spheres have average diameters of ca. 350 nm, and the wall thickness around the shell is about 42 nm. The possible formation mechanism of hollow Co₃O₄ spherical structures has simply been proposed.     

A citrate complex process to prepare nanocrystalline PbBi2Nb2O9 at a low temperature

PbBi₂Nb₂O₉ nanocrystals with a perovskite-type structure were successfully synthesized at a relative low temperature via a citrate complex method. Metal ions were dispersed by citric acid in ethanol and ethylene glycol solvent, and then reacted with NH₄H₂[NbO(C₂O₄)₃·3H₂O] to form the gel. XRD results showed that pure PbBi₂Nb₂O₉ nanocrystals could be obtained after calcined treatment of xerogel at 800 °C. The average particles size was 57 nm. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) revealed that the sintering process led to the agglomeration of the nanoparticles. The photocatalytic test showed that the sample prepared by the citrate complex method exhibited a higher photocatalytic activity than that of the sample prepared by the solid-state reaction.     

Synthesis and electrochemical properties of Co3O4 nanofibers as anode materials for lithium-ion batteries

Co₃O₄ nanofibers as anode materials for lithium-ion batteries were prepared from sol precursors by using electrospinning. The morphology, structure and electrochemical properties of Co₃O₄ nanofibers were characterized by atomic force microscopy (AFM), scanning electron microscopy (SEM), X-ray diffraction (XRD) and charge-discharge experiments. The results show that Co₃O₄ nanofibers possessed typical spinel structure with average diameter of 200 nm. The initial capacity of Co₃O₄ nanofibers was 1336 mAhg^− 1 and the capacity reached 604 mAhg^− 1 up to 40 cycles. It was suggested that the high reversible capacity could be ascribed to the high surface area offered by the nanofibers' structure.     

A facile hydrothermal route to spinel CoCo2O4 nanotubes and porous nanostructures without assisted surfactants and templates

Spinel CoCo₂O₄ nanotubes and porous nanostructures have been synthesized by a novel hydrothermal method from Co(NO₃)₂·6H₂O in mixtures of ammonia and cyclohexane at 220 °C. The morphology and phase of CoCo₂O₄ can be controlled by adjusting the experimental parameters that include the Co²⁺ concentration and the volume ratio of ammonia to cyclohexane. X-ray diffraction and transmission electron microscopy analyses were used to characterize the products. The formation mechanisms of CoCo₂O₄ nanostructures is proposed in detail. The electrochemical properties of the as-prepared samples have been investigated.     

Synthesis and characterization of Co3O4/RuO2 composite nanofibers fabricated by an electrospinning method

Co₃O₄-RuO₂ composite nanofibers (NFs) were synthesized by an electrospinning method and were calcinated at 400°C for 1 hr in air. Scanning electron microscopy and high-resolution transmission electron microscopy (HRTEM) examinations show that all the synthesized NFs have uniform surface morphology and their diameters are in the range of ~ 30-~70 nm. X-ray diffraction (XRD) results show that crystalline Co₃O₄ phase and RuO₂ phase coexist in the composite NF matrix which is confirmed by X-ray photoemission spectroscopy. In addition, the HRTEM energy-dispersive X-ray spectroscopy mapping results show that the Co₃O₄ and RuO₂ phases are uniformly distributed across the NF matrix.     

Fabrication of Co3O4 cubic nanoframes: Facet-preferential chemical etching of Fe ions to Co3O4 nanocubes

The novel Co₃O₄ cubic nanoframes, sized in ca. 30 nm, were firstly fabricated via a facile solvothermal route. Based on the transmission electron microscopy and the powder X-ray diffraction analyses of the time-dependent products, a mechanism of facet-preferential chemical etching of Fe³⁺ ions to the pre-synthesized Co₃O₄ nanocubes is proposed for the formation of Co₃O₄ cubic nanoframes. This synthetic strategy can probably be extended to fabricate nanoframes of some other binary metal oxides, by designing similar chemical etching process.     

Molten salt synthesis of single-crystal Co3O4 nanorods

The synthesis of the single-crystal Co₃O₄ nanorods by molten salt approach was reported for the first time. The products were characterized by Transmission electron microscopy (TEM), X-ray diffraction (XRD), High-resolution transmission electron microscopy (HRTEM) and Selected-area electron diffraction (SAED). TEM results indicate that these nanorods have diameters of about 150 nm and lengths of about 2 μm. According to the analysis of the SAED and HRTEM results, we drew the conclusion that these nanorods grew along an unusual [− 1,− 1,15] direction by Ostwald ripening mechanism.     

Photoluminescence properties of the In2O3 octahedrons synthesized by carbothermal reduction method

In₂O₃ octahedrons were synthesized by carbothermal reduction method. The products were characterized by X-ray diffraction (XRD), energy dispersive X-ray (EDX), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected-area electron diffraction analysis (SAED) and room-temperature photoluminescence (PL) spectra. The results show that the products are single-crystalline In₂O₃ octahedrons with the arrises length in the range of 400-3000 nm. The PL spectra displays blue and green emission peaks which can be indexed to default and oxygen vacancies; blue-shift and intensity decrease was observed when excitation wavelength decreases from 380 nm to 325 nm. The growth mechanism of the In₂O₃ octahedrons is discussed.     

Synthesis of K6Ta10.8O30 nanowires by molten salt technique

The synthesis of single crystalline K₆Ta_10.8O₃₀ nanowires by molten salt method was reported for the first time. X-ray diffraction results indicated that the as-prepared products were pure phase K₆Ta_10.8O₃₀. Scanning electron microscopy and transmission electron microscopy results showed that the products consisted of wire-like nanostructures with 100-300 nm in diameter and several micrometers in length. High resolution electron microscopy and selected area electron diffraction results indicated that the K₆Ta_10.8O₃₀ nanowires were single crystalline with a growth direction of [0 0 1]. The ultraviolet-visible diffuse reflectance measurement showed that the band gap of the nanowires was about 4.1 eV. The effects of reaction temperature, time, and weight ratio of the precursor (mixture of K₂CO₃ and Ta₂O₅) to KCl salt on the morphology of the products were investigated.     

Hydrothermal synthesis and characterization of LiNbO3 crystal

Lithium niobate crystal was successfully synthesized via hydrothermal synthesis method using LiOH·H₂O or LiNO₃ and Nb₂O₅ as starting materials in water or ammonia solution. X-ray diffraction (XRD), Fourier-transform infrared (FT-IR) spectra and Scanning electron microscopy (SEM) were used to characterize the as-prepared samples. The synthesis conditions such as crystallization temperature and time as well as ammonia concentration (when using LiNO₃ as Li source) were investigated. The results demonstrate that the crystallization and purity of the as-prepared samples were increased with the increase of time when temperature was at 260 °C. When using LiNO₃ as Li source a basic solution was necessary to synthesize LiNbO₃. In the present work ammonia solution was used instead of water to obtain alkalescence solvent. XRD results revealed that the as-prepared samples had a hexagonal structure. FT-IR results displayed that the LiNbO₃ phase could be completely formed and no secondary phase was found under proper conditions. SEM picture showed that the morphology of the sample was more perfect and bigger with increasing reaction time.     

Hydrothermal synthesis of Fe3O4 nanoparticles and its application in lithium ion battery

Well dispersed Fe₃O₄ nanoparticles with a mean diameter of about 160 nm were synthesized by a simple hydrothermal method in the presence of sodium sulfate. The products were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Raman spectrum, and Fourier transform infrared spectra (FTIR). Electrochemical properties of the nanostructured Fe₃O₄ as cathode electrodes of lithium ion battery were studied by conventional charge/discharge tests, showing a high initial discharge capacity of 1267 mA h g^− 1 at a current density of 0.1 mA cm^− 2.     

Polymer-assisted synthesis of Co2P nanocrystals

Co₂P nanocrystals were successfully synthesized by a polymer-assisted hydrothermal method. The reaction was carried out at 190 °C-220 °C using cobalt chloride hexahydrate (CoCl₂·6H₂O) as Co-source and yellow phosphorous as P-source. Polyacrylamide (PAM) was used as surfactant. By controlling the experiment parameters such as the reaction temperature and the amount of polyacrylamide (PAM), Co₂P nanocrystals with the rod-like or flower-like morphology could be prepared successfully. The phase and the morphology of the samples were characterized by X-ray diffraction (XRD), transmission electron microscopes (TEM), electron diffraction pattern (ED) and high resolution transmission electron microscope (HRTEM). Furthermore, based on the results of the TEM observation, the possible formation processes of the Co₂P nanorods or nanoflowers were also discussed.     

Synthesis and electrocatalytic property of mono-dispersed Ag/Fe3O4 composite micro-sphere

One-step reaction was designed to synthesize mono-dispersed Ag/Fe₃O₄ micro-sphere with different Ag content via a facile and easily controlled hydrothermal method without use of any surfactant. The phases and composition analysis of the as-prepared samples were characterized by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), respectively. The morphology of the samples was observed by transmission electron microscopy (TEM) and field-emission scanning electron microscopy (FE-SEM). The results revealed that the Ag/Fe₃O₄ composite samples with different Ag content were micro-spheres with almost the identical size of 175 nm or so in diameter. The electrocatalytic activity of the resultant samples modified on a glassy carbon electrode (GCE) for p-nitrophenol reduction in a basic solution was investigated. The results indicated that all the samples exhibited enhanced electrocatalytic activity for p-nitrophenol reduction, and the sample with 3% Ag exhibited the highest electrocatalytic one.     

Hydrothermal synthesis and characterization of monodisperse α-Fe2O3 nanoparticles

Monodisperse α-Fe₂O₃ nanoparticles have been successfully prepared by hydrothermal synthetic route using FeCl₃, CH₃COONa as reagents and reacted at 200 °C for 12 h. The morphology and structure of products were characterized by powder X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The results showed that the α-Fe₂O₃ nanoparticles were single-crystalline hexagonal structure and average diameters were about 80 nm. Magnetic properties have been detected by a vibrating sample magnetometer at room temperature. The nanoparticles exhibited a ferromagnetic behavior with the coercive force (Hc), saturation magnetization (Ms) and remanent magnetization (Mr) was 185.28 Oe and 0.494 emu/g, 0.077 emu/g.     

Synthesis and electrochemical properties of nanostructured LiMn2O4 for lithium-ion batteries

Spinel LiMn₂O₄ crystal with the grain sizes of about 15 nm is firstly synthesized by hydrothermal route at 180 °C using MnO₂ as a precursor. The LiMn₂O₄ powders synthesized by hydrothermal technique and sol-gel reaction were investigated by X-ray diffraction (XRD) and Transmission electron microscopy (TEM). The LiMn₂O₄ samples were used as cathode materials for lithium-ion battery, whose electrochemical properties were investigated. The results show that the sample obtained by hydrothermal route has higher capacity than that prepared by sol-gel method.     

Synthesis of nano-particles of anatase-TiO2 and preparation of its optically transparent film in PVA

Anatase-TiO₂ nano-particles have been synthesized by using long-carbon chain carboxylic acid and titanium tetrachloride (TiCl₄). As-prepared powder has been calcined at 500 °C to obtain highly crystalline TiO₂. Broad X-ray diffraction (XRD) pattern of as-prepared as well as calcined powder showed all prominent peaks for tetragonal crystal structure representing anatase-TiO₂. The particle diameter by applying Scherrer formula was found to be about 20 nm. It was possible to load as-prepared particles in poly vinyl alcohol (PVA) for optical studies. Optically transparent film showed sharp absorption band for TiO₂ nano-particles at ∼ 300 nm. Photoluminescence (PL) studies of the solution showed emission wavelength at about 330 nm. Transmission electron microscopy (TEM) and selected area electron diffraction (SAED) revealed that the particles in the film have uniform distribution and even for the powder no agglomeration was observed. Thermal analysis (TGA) showed that the stability of host polymer is enhanced. FTIR spectra showed presence of carboxylate functional group in the powder.     

Solvothermal synthesis of In(OH)3 nanorods and their conversion to In2O3

In this work, we demonstrate that monodisperse indium hydroxide (In(OH)₃) nanorods constructed with parallel wire-like subunits have been fabricated via a acrylamide-assisted synthesis route without any template. NH₃ from the hydrolysis of acrylamide acts as the OH⁻ provider. The structure and morphology of as-prepared products have been characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM) and thermogravimetric analysis (TG). A detailed mechanism has been proposed on the basis of time-dependent experimental results. Furthermore, by annealing In(OH)₃ precursors at 500 °C for 3 h in air, In₂O₃ samples were obtained with the designed morphology.     

Solvothermal synthesis of sheet-like Co3O4 and Ag/Co3O4 nanocomposites and their electrocatalysis performances

Precursors of Co₃O₄ and Ag/Co₃O₄ composites with sheet-like shape were synthesized with assistance of ethylene glycol via a solvothermal process. The final samples were obtained by calcining each precursor at 400 °C. The as-prepared samples were identified and characterized by thermogravimetric analysis (TG) and differential thermal gravimetric (DTG) analysis, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), and field emission scanning electron microscopy (FE-SEM). The Co₃O₄ and Ag/Co₃O₄ composite nanosheets were used as electrocatalysts modified on a glassy carbon electrode for p-nitrophenol and H₂O₂ reduction respectively in a basic solution. The electrocatalytic results showed that p-nitrophenol could be reduced by pure Co₃O₄ at a large peak current but a rather higher peak potential, and could be reduced effectively by Ag/Co₃O₄ composites at lower potential. Ag/Co₃O₄ composites with 6% Ag displayed the highest electrocatalytic activity for H₂O₂ reduction at the largest peak current and a lower peak potential. The reduction peak potentials of H₂O₂ all reduced a great deal using Ag/Co₃O₄ composite.     

Preparation and characterization of Co-doped ZnO-Al2O3-SiO2 glass-ceramics by the sol-gel method

Transparent glass-ceramics containing Co²⁺:ZnAl₂O₄ nanocrystals were obtained by the sol-gel process for the first time. The gels of composition 89SiO₂-5.9Al₂O₃-4.9ZnO-0.2CoO (ZAS) were prepared at room temperature, and heat-treated at different temperatures. The microstructure and optical properties of the heated samples were studied by using X-ray diffraction (XRD), transmission electron microscopy (TEM), infrared spectroscopy, and optical absorption spectra. Co²⁺:ZnAl₂O₄ nanocrystals were precipitated from ZAS system and dispersed in the SiO₂-based glass during heat-treatment in the temperature range 900-1100 °C. Co²⁺ ions were located in tetrahedral sites in ZnAl₂O₄ nanocrystals. The Co²⁺:ZnAl₂O₄ crystallite size was in the range of 4-15 nm.